CN105185431A - Superhigh protection silver conductive film preparation method - Google Patents

Superhigh protection silver conductive film preparation method Download PDF

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Publication number
CN105185431A
CN105185431A CN201510646956.3A CN201510646956A CN105185431A CN 105185431 A CN105185431 A CN 105185431A CN 201510646956 A CN201510646956 A CN 201510646956A CN 105185431 A CN105185431 A CN 105185431A
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substrate
minutes
silver
preparation
djb
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CN105185431B (en
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程江
陈善勇
李璐
刘碧桃
金容�
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Shenzhen Texin Interface Technology Co ltd
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Chongqing University of Arts and Sciences
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Abstract

The invention discloses a superhigh protection silver conductive film preparation method, comprising the steps of: cleaning, drying and plasma processing a substrate; coating and drying a layer of DJB-823 solid film protective agent on the substrate to obtain a silver conductive network after drying; coating silver nanowire conductive ink on a tie coat to obtain a silver conductive network after drying; and coating the DJB-823 solid film protective agent on a conductive network, and performing drying to obtain a superhigh protection silver conductive film. The conductive film wins the second prize of national innovation, is widely applied to the DJB-823 solid film protective agent in aeronautics and astronautics and military supplies, can keep sound resistance to the stimulation of a plurality of environments, and reach excellent levels in various performances, and is widely used in the electronic information field.

Description

A kind of preparation method of silver-colored conductive film of superelevation protection
Technical field
The invention belongs to transparent conductive film technical field, be specifically related to the preparation of the silver-colored conductive film of a kind of superelevation protection.
Background technology
At present, use maximum electrode materials to be tin indium oxide (ITO), and the material most possibly realizing commercialization flexible electrode is nano silver wire.Nano silver wire is mixed with ink by people, is then coated in the substrate of primary coat tack coat by modes such as spraying, blade coating, roller coating by ink, is finally coated on silver nanoparticle network by top stopping off, obtains silver-colored conductive film.Primary coat and top be coated with use considerably increase silver-colored conductive film barrier propterty and significantly improve membrane life time, make its from practical more and more close to.Conventional basecoat material is various resin mainly, as epoxy resin, acrylic resin, polyurethane etc.Conventional top is coated with material and mainly contains UV glue, optical cement, various resin, conducting polymer etc., as described in patent CN104658700A, CN102522145A, CN102522145B.But these primary coats and top be coated with material have a common drawback: the barrier propterty stimulated to external world not enough and coating the part of dargyrome network performance can be caused to decline.This is wrapped in silver-colored line surface by macromolecular material and hinders dargyrome network conduction and the barrier propterty decision of macromolecule own.Obtain superelevation protection high-performance silver conductive film, need there is superelevation barrier propterty and do not affect Thin film conductive performance protection binding agent occur.And this kind of research does not also occur in the patent.
Therefore, finding suitable protection binding agent, to prepare the high-performance silver conductive film with superelevation barrier propterty be the problem that solution is needed in conductive film field badly.
Summary of the invention
The preparation of the silver-colored conductive film that the object of the present invention is to provide a kind of superelevation to protect, the problem that solution current thin film barrier propterty is not enough and protective agent causes dargyrome network electric conductivity to decline.This film has that barrier propterty is super good, conductivity is high, light transmittance is high, with the advantage such as substrate associativity is good, preparation simply, can be widely used in electronic information field.Its specific embodiments is:
(1) substrate is carried out clean, dry and plasma treatment;
(2) on substrate, apply one deck DJB-823 solid film protective agent, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) DJB-823 solid film protective agent is coated on conductive network, after oven dry, obtains the silver-colored conductive film of a kind of superelevation protection.
The substrate that the present invention uses is the one in PETG (PET), dimethyl silicone polymer (PDMS), Merlon, polyimides (PI) or glass;
(1) in substrate cleaning, dry with plasma treatment process be: the diaphragm newly bought on substrate is torn off, puts it in acetone, ethanol and distinguish ultrasonic 5 minutes.Then substrate infrared baking lamp is toasted 5 minutes.Take out substrate, put it in plasma cleaner, vacuum cleaned 5 minutes.Wherein, the power of the infrared baking lamp of use is 800W, drying area is 1000cm 2; Frequency/the power of the plasma cleaner used is 13.56MHz/300W;
The substrate that (1) processed applies one deck DJB-823 solid film protective agent solution, makes the thickness after oven dry at about 300nm.Coating uses GardcoAutomaticDrawdownMachineDP8301 sheet type coating machine, also comprises other coating machines.After having applied, first toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes;
(2) in, the preparation steps of DJB-823 solid film protective agent solution is: DJB-823 solid film protective agent is whittled into powder, takes 0.5-2 gram, add in 100ml mixed solvent (No. 120 industrial napthas 60%, n-butanols 40%).Be heated to 55-65 DEG C in a water bath and stir 10 minutes gently.To be protected dose be dissolved into clear solution completely after, keep bath temperature 50-65 DEG C can use;
(2) basis applies last layer nano silver wire coating fluid.Then, first 3 minutes are toasted with infrared baking lamp.Then to use at vacuum drying oven 110 DEG C vacuumize 10 minutes, obtain the nano silver wire network that thickness is about 200nm.Nano silver wire ink is homemade.Nano silver wire diameter is between 30-50nm, and length is between 10-20 μm.Ink silver line content is about 0.5%.Except silver-colored line, ink is also containing auxiliary agents such as dispersant, surfactant, levelling agent, NMF and binding agents;
(4) be coated on silver-colored conductive network by DJB-823 solid film protective agent solution in, control coated weight makes the thickness after oven dry at about 150nm.Then first toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, obtain the final silver-colored conductive film having superelevation barrier propterty;
The present invention uses widely used DJB-823 solid film protective agent in Aero-Space and military products.Its stable in physicochemical property, nontoxic, odorlessness, in an atmosphere nonhygroscopic, do not decompose, do not distil, do not adsorb flying dust and pernicious gas, can long-term storage.It is super good to the barrier propterty of the especially silver-colored based article of metal, the superpower protection 5-10 of energy, and general guard time is longer.This protective agent has splendid bond properties to metal and plastics, silver-colored line and substrate can be adhered to each other firmly.Meanwhile, experiment shows, this protective agent does not even also almost affect the performance such as conductivity, the insulating properties of plastics, the high frequency of waveguide component of metal when a few micron thickness.Which ensure that and be coated in after on silver nanoparticle network, the conductivity of silver nanoparticle network will not reduce;
The present invention has the following advantages: the film that the protectant use of (1) DJB-823 solid film makes the present invention prepare has the barrier propterty of superelevation, can resist the various stimulations of external environment; (2) its super good adhesive property is super good by the caking property of conductive network and substrate; (3) after its coating, the conductivity of dargyrome network is not affected, ensure that the conductivity that film of the present invention is good; (4) filling between dargyrome network decreases the scattering of light, and thus product mist degree is low; (4) film light transmittance is high.These ensure that film of the present invention can widely use at electronic information field.
Accompanying drawing explanation
Fig. 1: structural representation of the present invention;
1-substrate; 2-DJB-823 solid film protective agent tack coat; 3-silver conductive network; 4-DJB-823 solid film protective agent protective layer; Wherein, 3 and 4 layers overlap.
Specific embodiment
Embodiment:
Adopt PET as substrate.Diaphragm on new substrate is torn off, puts it in acetone, ethanol and distinguish ultrasonic 5 minutes.Then dry with infrared baking lamp.Then put it in plasma cleaner, vacuum cleaned 5 minutes;
DJB-823 solid film protective agent is whittled into powder, takes 0.5-2 gram, add in 100ml mixed solvent (No. 120 industrial napthas 60%, n-butanols 40%).Be heated to 55-65 DEG C in a water bath and stir 10 minutes gently.To be protected dose be dissolved into clear solution completely after, keep bath temperature 50-65 DEG C stand-by;
With GardcoAutomaticDrawdownMachineDP8301 sheet type coating machine coating last layer DJB-823 solid film protective agent solution on the substrate processed.Then, first toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes.Obtain the tack coat of a layer thickness in about 300nm left and right;
Tack coat applies one deck nano silver wire solution, first toasts 3 minutes with infrared baking lamp, then to use at vacuum drying oven 110 DEG C vacuumize 10 minutes, obtain the nano silver wire network of thickness at about 200nm;
DJB-823 solid film protective agent solution is coated on silver-colored conductive network.First toast 3 minutes with infrared baking lamp, then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, obtain the protective layer that 150nm is thick.Comprehensive above each step obtains the final silver-colored transparent conductive film having superelevation barrier propterty.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.All technical staff in the art, all should by the determined protection range of claims under this invention's idea on the basis of existing technology by the available experiment of logical analysis, reasoning, or a limited experiment and technical scheme.

Claims (8)

1. a preparation method for the silver-colored conductive film of superelevation protection, it is characterized in that, concrete preparation process is:
(1) substrate is carried out clean, dry and plasma treatment;
(2) on substrate, apply one deck DJB-823 solid film protective agent, dry;
(3) nano silver wire conductive ink is coated on tack coat, after drying, obtains silver-colored conductive network;
(4) DJB-823 solid film protective agent is coated on conductive network, after oven dry, obtains the silver-colored conductive film of a kind of superelevation protection.
2. preparation method according to claim 1, is characterized in that: substrate is the one in PETG (PET), dimethyl silicone polymer (PDMS), Merlon, polyimides (PI) or glass.
3. preparation method according to claim 1, is characterized in that: in (1), the cleaning of substrate is torn off by the diaphragm on substrate, then substrate is put into acetone, ethanol ultrasonic 5 minutes respectively; Drying is toasted 5 minutes under the substrate after cleaning being placed on infrared baking lamp.
4. preparation method according to claim 1, is characterized in that: the plasma treatment process of step (1) is: by lying substrate in plasma processor, opens machine to substrate processing 5 minutes.
5. preparation method according to claim 1, it is characterized in that: the preparation steps of the DJB-823 solid film protective agent solution in step (2) is: DJB-823 solid film protective agent is whittled into powder, take 0.5-2 gram, add in 100ml mixed solvent (No. 120 industrial napthas 60%, n-butanols 40%); Be heated to 55-65 DEG C in a water bath and stir 10 minutes gently; To be protected dose be dissolved into clear solution completely after, keep bath temperature 50-65 DEG C can use.
6. preparation method according to claim 1, is characterized in that: the oven dry of step (2) for first to toast 5 minutes with infrared baking lamp, then in vacuum drying oven at 100 DEG C, vacuum dry 10 minutes.
7. preparation method according to claim 1, is characterized in that: step (3) nano silver wire used is homemade, and diameter is between 30-50nm, and length is between 10-20 μm; Ink silver line content is about 0.5%; Except silver-colored line, ink is also containing dispersant, surfactant, levelling agent, NMF and binding agent etc.; After ink coating, first toast 3 minutes with infrared baking lamp; Then substrate is put into vacuum drying oven, heated baking 10 minutes at 110 DEG C, vacuum.
8. preparation method according to claim 1; it is characterized in that: after DJB-823 solid film protective agent solution applies by step (4); 3 minutes are first toasted with infrared baking lamp; then with baking under vacuum drying oven 100 DEG C of vacuum 10 minutes, the silver-colored conductive film of final superelevation protection is obtained.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106927693A (en) * 2017-01-19 2017-07-07 广东南海启明光大科技有限公司 A kind of nano-silver thread transparent conducting glass and preparation method thereof
CN108565042A (en) * 2018-04-24 2018-09-21 河南省豫星华晶微钻有限公司 A kind of conductive and heat-conductive electric slurry and preparation method thereof containing nanometer diamond alkene

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Publication number Priority date Publication date Assignee Title
CN1978388A (en) * 2005-12-03 2007-06-13 深圳振华富电子有限公司 Surface protection treatment method for electronic ceramic chip type element
CN102087886A (en) * 2009-12-08 2011-06-08 中国科学院福建物质结构研究所 Silver nanowire-based transparent conductive thin film and preparation method thereof
CN104112544A (en) * 2014-05-14 2014-10-22 中国科学院合肥物质科学研究院 Preparation method for silver nano wire transparent conductive film capable of preventing corrosion of hydrogen sulfide gas
WO2015068654A1 (en) * 2013-11-05 2015-05-14 昭和電工株式会社 Conductive pattern formation method, production method for on-cell-type touch panel using same, transfer film used in same, and on-cell-type touch panel
CN104919011A (en) * 2013-01-22 2015-09-16 东进世美肯株式会社 Transparent conductive film coating composition, transparent conductive film, and method for manufacturing transparent conductive film

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1978388A (en) * 2005-12-03 2007-06-13 深圳振华富电子有限公司 Surface protection treatment method for electronic ceramic chip type element
CN102087886A (en) * 2009-12-08 2011-06-08 中国科学院福建物质结构研究所 Silver nanowire-based transparent conductive thin film and preparation method thereof
CN104919011A (en) * 2013-01-22 2015-09-16 东进世美肯株式会社 Transparent conductive film coating composition, transparent conductive film, and method for manufacturing transparent conductive film
WO2015068654A1 (en) * 2013-11-05 2015-05-14 昭和電工株式会社 Conductive pattern formation method, production method for on-cell-type touch panel using same, transfer film used in same, and on-cell-type touch panel
CN104112544A (en) * 2014-05-14 2014-10-22 中国科学院合肥物质科学研究院 Preparation method for silver nano wire transparent conductive film capable of preventing corrosion of hydrogen sulfide gas

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106927693A (en) * 2017-01-19 2017-07-07 广东南海启明光大科技有限公司 A kind of nano-silver thread transparent conducting glass and preparation method thereof
CN108565042A (en) * 2018-04-24 2018-09-21 河南省豫星华晶微钻有限公司 A kind of conductive and heat-conductive electric slurry and preparation method thereof containing nanometer diamond alkene
CN108565042B (en) * 2018-04-24 2020-02-07 河南省豫星微钻有限公司 Electric-conduction and heat-conduction electronic paste containing nano diamond alkene and preparation method thereof

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Effective date of registration: 20220624

Address after: 518107 C501, building A3, Guangming Science Park, China Merchants Group, sightseeing Road, Fenghuang community, Fenghuang street, Guangming District, Shenzhen City, Guangdong Province

Patentee after: Shenzhen Texin Interface Technology Co.,Ltd.

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